Soft magnetic thin films of Ni, NiFe and NiFe2O4 were prepared using reactive magnetron sputtering in various deposition conditions. Experimentally observed soft magnetic property was compared and correlated with nanocrystalline structure evolution. Ni and NiFe deposited films are textured with fcc(111) phase preferred orientation. Accordingly, grain size and lattice parameter were calculated from X-ray diffraction (111) peak line width and 2θ peak position. Addition of reactive gas oxygen in deposition process has substantial effect on crystalline structure of film. There is phase transition from the ordered NiFe (111) structure to the NiFe2O4 nanocrystalline phase. The resulting film has shown small X-ray diffraction intensity peak corresponding to (311) and (400) orientation, indicating small amount of existing NiFe2O4 phase. The mechanism has been discussed to be responsible for nanocrystallization and amorphization of NiFe2O4 films. Magnetic measurement (M-H) loop reveal soft magnetic nature of films with magnetic anisotropy. The coercivity (Hc) of films is in accordance with random anisotropy model, where Hc reduced with grain size. The structural transformation was supported by Fourier transforms infrared spectroscopy measurement. The films are highly smooth with surface roughness in the range of ∼0.53–0.93nm. NiFe2O4 films have shown lowest surface roughness with highest electrical resistivity values. The structural, surface, magnetic and infrared spectroscopy results are observed and analyzed.